Perfluormethyl-Element-Liganden, XXI [1]. Darstellung und Charakterisierung von Organoelement-Element-Verbindungen des Typs R_nE–ER_m (R = CH₃, CF₃; E = P, As, S, Se, Te; n,m = 1, 2) / Perfluoromethyl Element Ligands, XXI [1]. Preparation and Characterization of Organoelement Element Compounds of the Type R_nE–ER_m (R = CH₃, CF₃; E = P, As, S, Se, Te; n,m = 1, 2)

Abstract

<jats:p>Element-element compounds of the general type R<jats:sub>n</jats:sub>E-ER<jats:sub>m</jats:sub> (R = CH<jats:sub>3</jats:sub>, CF<jats:sub>3</jats:sub>; E = P, As, S, Se, Te; n,m = 1, 2) have been prepared by different synthetic methods. New compounds were characterized by analytical and spectroscopic (NMR, MS) investigations. Information about the most suitable preparative route for all possible combinations is given in Tables I to III.</jats:p>

Analysis of volatile arsenic compounds formed by intestinal microorganisms: rapid identification of new metabolic products by use of simultaneous EI-MS and ICP-MS detection after gas chromatographic separation

“…Finally, the boiling point of the compound, estimated on the basis of the retention time index, is very close to the reported value (Table 1). In contrast, Me 3 As]S has a melting point of 170 C. 10 Me 2 AsSMe has already been detected in compost samples and hydrothermal gas from Yellowstone National Park by K€ osters et al 14 and Planer-Friedrich et al 15 The second most abundant peak in the chromatogram was assigned to Me 2 AsSH (dimethyl-mercapto-arsine or dimethylthioarsinous acid), which has been detected in rat liver homogenates by HPLC-ESI-MS. 3 The mass spectrum (Fig. 2a) shows the main fragments at m/z 138 and 123, which arise from the molecular ion and the demethylated fragment ion, respectively.…”

“…Synthesis of mixed arsenic/sulfur and mixed arsenic/selenium species In order to synthesize mixed arsenic/sulfur species, a preparation according to Dehnert et al was carried out. 10 293 mg (12 mmol) of magnesium chips (Merck-Schuchardt, Munich, Germany) were placed in a 20 mL reaction vial cooled by liquid nitrogen. Then, 50 ml of methyl mercaptan (98%, Fluka, Steinheim, Germany) and 23 mg (0.1 mmol) of Me 2 AsI were added.…”

“…2c. The compound was identified as Me 2 AsSMe (dimethyl-methylthio-arsine) by comparison with spectra from the literature 10,12 as well as by spectrum and retention time comparison with synthesised Me 2 AsSMe (Fig. 2d).…”

“…2e and 2f, the fragmentogram of the arsenic compound at 5.9 min retention time is presented, which was identified as Me 2 AsSeMe (dimethyl-methylseleno-arsine) by comparison with literature spectra. 10 The presence of selenium in this compound was indicated by the 77 Se-and 82 Se-ICP-MS mass traces showing a peak at the same retention time (see Fig. S1, ESI) † as well as by the EI-MS spectrum, which shows the typical isotopic pattern of selenium ( 74 Se: 0.87%, 76 Se: 9.36%, 77 Se: 7.63%, 78 Se: 23.78%, 80 Se: 49.61%, 82 Se: 8.73%).…”

Verbindungen des Typs (F3C)2EE′R mit Pseudohalogen-Charakter (E = P, As; E′ = S, Se, Te)

“…Voraussetzung dafu È r ist eine hohe Polarita È t der EE'-Bindung, die eine ausreichende ¹ionische Resonanzenergieª garantiert. Gute Ergebnisse wurden in unserer Arbeitsgruppe fu È r einige der gewu È nschten Verbindungen bereits Ende der 70er Jahre erzielt [6]. Ûber fru È -here Beispiele [Me 2 AsSCF 3 bzw.…”